Construction method and applications of tussilago farfara l liquid phase fingerprint
A technology of fingerprint spectrum and construction method, which can be used in measurement devices, instruments, scientific instruments, etc., can solve problems such as reflecting the quality of medicinal materials, and achieve the effects of good reproducibility, accurate evaluation and simple pretreatment.
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Embodiment 1
[0031] The determination of embodiment 1 chromatographic conditions and the designation of characteristic peaks
[0032] 1. Selection of mobile phase
[0033] Five kinds of mobile phase systems were selected in the experiment: methanol-water, acetonitrile-water, acetonitrile-0.03% acetic acid water, acetonitrile-0.03% formic acid water, 0.03% formic acid acetonitrile-0.03% formic acid water for HPLC of Coltsfoot flower Determination. as attached figure 1 As shown, seven higher chromatographic peaks can be seen in both the methanol-water system and the acetonitrile-water system, but the chromatographic peaks appear later in the methanol-water system, and the number of characteristic chromatographic peaks in the acetonitrile-water system is less ; The baseline drift is more serious in the acetonitrile-0.03% acetic acid water system and the acetonitrile-0.03% formic acid water system, and the resolution of each peak in the acetonitrile-0.03% acetic acid water system is low and ...
Embodiment 2
[0046] Embodiment 2 Fingerprint Atlas Methodological Investigation
[0047] The need testing solution of following experiment all adopts following method preparation:
[0048] Extract 1.0 g of winter flower powder, add 20 mL of 75% methanol, ultrasonically extract for 1 hour, make up the lost weight with 75% methanol, and pass the solution through a 0.22 μm microporous membrane to obtain the test solution.
[0049] Precision experiment:
[0050] Extracting winter flower medicinal material (SX-9), continuous sample injection 6 times, using No. 12 peak as reference peak, record the relative retention time and relative peak area of other characteristic peaks, the result shows that the RSD of the relative retention time of each chromatographic peak is in 0.02% to 0.66%; the RSD of the relative peak area is 0.60% to 2.05%, indicating that the test solution of Coltsfoot flower is analyzed by high performance liquid chromatography, and the precision of the whole detection system i...
Embodiment 3
[0055] Example 3 Comparison of Coltsfoot Flower Liquid Fingerprints from Different Places of Origin
[0056] 26 batches of coltsfoot medicinal materials from different origins (Table 1) were determined using the liquid fingerprint conditions of coltsfoot flower established above.
[0057] Extract 1.0 g of winter flower powder, add 20 mL of 75% methanol, ultrasonically extract for 1 h, make up for the lost weight with 75% methanol, pass the solution through a 0.22 μm microporous membrane, and take the subsequent filtrate to obtain the test solution. The chromatographic column Venusil MP (250mm×4.6mm, 5μm) was used as the stationary phase, and the test was carried out according to the following liquid phase conditions:
[0058] UV detection wavelength is 254nm / 220nm switching detection; column temperature is 25°C; injection volume is 10μL; flow rate is 1mL / min; gradient elution conditions are 0-2min, 5% A phase; %A phase; 7-35min, 15%-30%A phase; 35-38min, 30%-55%A phase; 38-45...
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